Synthetic method of p-methylphenyl oxyethyl methyl ether
A technology of toluene oxyethyl methyl ether and a synthesis method, which is applied in the directions of ether preparation, organic chemistry and the like, can solve the problems of high price, unfavorable development of the daily chemical industry, etc., and achieves low production cost, easy control of synthesis process conditions, and good activity. Effect
Inactive Publication Date: 2016-02-10
尹建明
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Problems solved by technology
[0003] The purpose of the present invention is to solve the problem that the tolyloxyethyl methyl ether currently used in industry in my country mainly relies on imports, is expensive, and is not conducive to the development of my country's daily chemical industry, and provides a synthetic method of p-tolyloxyethyl methyl ether
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Effect test
Embodiment 1
[0010] A kind of synthetic method of p-tolyloxyethyl methyl ether of the present invention comprises the following steps:
[0011] (1) Add p-toluene, potassium hydroxide and absolute ethanol into the reaction kettle, heat and stir to dissolve them, then add chloroethanol, heat, and react at 50-55°C for 8 hours, waxy solids are continuously precipitated during the reaction , then heated to boiling, refluxed for 15 minutes, cooled, and suction filtered. The filtrate was first distilled to ethanol at normal pressure, and then distilled under reduced pressure to collect fractions at 118-121°C to obtain p-tolyl glycol monoether;
[0012] (2) Take the p-tolyl glycol monoether prepared in the previous step, dissolve it in ether, heat the catalyst 2PBBC, add 50% sodium hydroxide solution while stirring, stir and react for 15 minutes, after cooling to room temperature, add sulfuric acid dropwise Dimethyl ester, the rate of addition is controlled so that the reaction temperature does no...
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The invention discloses a synthetic method of p-methylphenyl oxyethyl methyl ether, which includes the following steps: 1) adding p-toluene, potassium hydroxide and anhydrous ethanol into a reaction kettle, heating and stirring the mixture to dissolve the components; 2) adding chloroethanol, carrying out a heating reaction for 8 h and reflux for 15 min, and performing cooling and suction filtration to obtain a filtrate, and treating the filtrate to obtain p-methylphenyl ethylene glycol monoether; 3) dissolving the p-methylphenyl ethylene glycol monoether in ethyl ether, adding a catalyst and a 50% sodium hydroxide solution, carrying out a stirring reaction for 15 min, cooling the reaction product to room temperature, dropwisely adding dimethyl sulfate, carrying out a stirring reaction below 40 DEG C for 10-12 h, and cooling the reaction product to room temperature; 4) adding concentrated ammonia water, stirring the mixture at room temperature for 0.5 h, adding water and regulating the pH to neutralization by means of sulfuric acid; 5) filtering the mixture to remove the catalyst, drying the filtrate, performing normal-pressure distillation to recycle the ethyl ether, and performing reduced-pressure distillation and collecting the fraction at 128-130 DEG C to obtain the product. The method is simple, is easy to control in technical conditions, is less in by-products, is low in cost and is a green and environment-friendly synthetic process route.
Description
technical field [0001] The invention relates to a synthesis method of perfume, in particular to a synthesis method of p-tolyloxyethyl methyl ether. Background technique [0002] P-cresyloxyethyl methyl ether is a new type of fragrance. This fragrance has a pleasant natural leafy green fragrance, which is similar to European clove, ylang-ylang and rose fragrance. It has been widely used in soaps, detergents, and household bleaches. , air conditioners, indoor sprays, facial cleansers, insect repellents, ointments, perfumes, shaving creams, powders, hair cosmetics, deodorants, and sweat inhibitors, etc. Fragrance effect. At present, the tolyloxyethyl methyl ether used in my country's industry mainly depends on imports, and the price is relatively high, which is not conducive to the development of my country's daily chemical industry. Therefore, it is a matter of great social significance to independently develop a synthetic method of p-tolyloxyethyl methyl ether. Contents o...
Claims
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IPC IPC(8): C07C43/23C07C41/01
Inventor 尹建明
Owner 尹建明